CN102580643A - Micro-reaction device and application thereof in synthesis of glycidyl methacrylate - Google Patents
Micro-reaction device and application thereof in synthesis of glycidyl methacrylate Download PDFInfo
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- CN102580643A CN102580643A CN201110455573XA CN201110455573A CN102580643A CN 102580643 A CN102580643 A CN 102580643A CN 201110455573X A CN201110455573X A CN 201110455573XA CN 201110455573 A CN201110455573 A CN 201110455573A CN 102580643 A CN102580643 A CN 102580643A
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Abstract
The invention discloses a micro-reaction device and application thereof in synthesis of glycidyl methacrylate. The micro-reaction device disclosed by the invention is at least composed of a device unit, wherein the device unit comprises a thermostatic oil bath, a discharge tank, at least two charge tanks I and II, a micro-mixer and a delayed reaction channel; the charge tank I is connected with the micro-mixer through a constant flow pump I; the charge tank II is connected with the micro-mixer through a constant flow pump II; the other side of the micro-mixer is connected with a receiver through the delayed reaction channel; and the delayed reaction channel is fixed in the thermostatic oil bath. When conveyed and transferred in a reaction system, the material in the micro-reaction device is in a closed state, so that operations for the reaction are safe. When the micro-reaction device is applied to a reaction of synthesizing the glycidyl methacrylate, reaction time and energy consumption are saved, and the reaction technology is amplified and ensured to be simple and convenient; and relative device investment and maintenance cost is low as regular chemical reaction devices, such as a reaction kettle and a condenser, are not needed.
Description
Technical field
The present invention relates to a kind of micro-reactor apparatus, and the application on the synthesize methyl acrylic acid glycidyl ester, chemical technology field belonged to.
Background technology
The GMA chemical name is methacrylic acid-beta epoxide propyl ester, and structural formula is:
GMA is a kind of colourless transparent liquid; Have two active function groups of epoxy radicals and carbon-carbon double bond; It is a kind of high activity synthon; In the acrylic resin paint of synthetic excellent performance, have important purposes, be widely used in fields such as organic synthesis, medicine, photosensitive material, polymer modification, coating, adhesive, rubber industry, printing-ink.
One-step synthesis is the main method of preparation GMA, the characteristics of this method be the reaction time short (2～4h), productive rate high (generally 92%～97%), good product quality is the external method that adopts at present.But this method requires whole reaction system anhydrous, and very high to the sodium salt purity requirement, the sodium salt water content is lower than 5%; The ester yield is reached more than 92%; And have epoxychloropropane consumption big (needing excessive 4～10 times), and this method reactions step is long, post processing is complicated.Two of the GMA of report step synthetic methods are a kind of synthetic methods with application prospect in the recent period.This method is raw material with the methacrylic acid, under catalyst and inhibitor action, carries out the esterification by ring opening reaction with epoxychloropropane; Carry out ring-closure reaction synthesize methyl acrylic acid glycidyl ester with NaOH then.This method has advantages such as the epoxychloropropane consumption is few, easy and simple to handle, environmental pollution is little.But this method has that the reaction time is long, and side reaction is many, can not produce continuously, and technology is amplified limitations such as difficulty.
Summary of the invention
The purpose of this invention is to provide a kind of micro-reactor apparatus, it has enlarge-effect simple in structure, no, operating condition is easy to advantages such as control and intrinsic safety.Use littlely to be reacted into little chemical process that complete equipment carries out and to have with continuous process and replace batch process, process intensification, security improves, and product property changes, advantages such as distributing production.
A kind of micro-reactor apparatus provided by the present invention is characterized in that being made up of a unit at least; Described unit comprises thermostatical oil bath and discharge tank and at least two head tank I, head tank II; Also comprise micro-mixer and time-delay reaction channel; Described head tank I through constant flow pump I link to each other with micro-mixer, head tank II links to each other with micro-mixer through constant flow pump II, the opposite side of micro-mixer links to each other with receiver through the reaction channel of delaying time, the reaction channel of delaying time is fixed in the thermostatical oil bath.
In the above-mentioned micro-reactor apparatus, further optimize its equipment, according to raw material properties, can micro-mixer be fixed in the thermostatical oil bath, the channel diameter of its micro-mixer is 50 μ m～600 μ m.
In the above-mentioned micro-reactor apparatus, for optimization further, the diameter of time-delay reaction channel is preferably 1.59mm～6.35mm, and length is preferably 30cm～500cm.The material of time-delay reaction channel is preferably stainless steel.
In the above-mentioned micro-reactor apparatus, described receiver is preferably the micro-mixer in discharge tank or next the said unit.
In the above-mentioned micro-reactor apparatus, preferred two said units; Micro-reactor apparatus head tank I through constant flow pump I link to each other with micro-mixer I, head tank II passes through constant flow pump II and links to each other with micro-mixer I; The opposite side of micro-mixer I links to each other with micro-mixer II through time-delay reaction channel I, and micro-mixer I and time-delay reaction channel I are fixed among the thermostatical oil bath I; Described head tank III links to each other with micro-mixer II through constant flow pump III, and the opposite side of micro-mixer II links to each other with receiver through time-delay reaction channel II, and micro-mixer II and time-delay reaction channel II are fixed among the thermostatical oil bath II.
Another object of the present invention provides a kind of method of synthesize methyl acrylic acid glycidyl ester, comprises esterification by ring opening reaction and ring-closure reaction, it is characterized in that said being reflected in above-mentioned arbitrary described micro-reactor apparatus carry out.
The method step of described synthesize methyl acrylic acid glycidyl ester is following:
1. esterification by ring opening reaction:
A joins epoxychloropropane among the head tank I; With methenamine and MEHQ be dissolved in the methacrylic acid mixture I, its mixture I is joined among the head tank II; Wherein, Epoxychloropropane and methacrylic acid in molar ratio 1.3～1: 1 feeds intake; The addition of methenamine is 0.5～1.0% of methacrylic acid and an epoxychloropropane gross mass, and the addition of MEHQ is 0.1～0.5% of methacrylic acid and an epoxychloropropane gross mass;
When b rises to 70～100 ℃ with the temperature of thermostatical oil bath; Open constant flow pump I and constant flow pump II; Flow velocity is 0.5ml/min～20ml/min; Enter into micro-mixer and mix, the inflow diameter is that 1.59mm～6.35mm, length are that the time-delay reaction channel of 30cm～500cm reacts, and the product I that obtains gets in the discharge tank;
2. ring-closure reaction:
A joins product I among the head tank I; Sodium hydrate aqueous solution is joined among the head tank II; Wherein, NaOH and methacrylic acid-2-hydroxyl-3-chlorine propyl ester in molar ratio 1.0～1.1: 1 feeds intake;
When b rises to 40 ℃ with the temperature of thermostatical oil bath, open constant flow pump I and constant flow pump II, enter into micro-mixer and mix, flow into the time-delay reaction channel and react, the product II that obtains gets in the discharge tank;
3. product II is separated, get oil reservoir, washing is to neutral, and drying gets GMA.
In the method for above-mentioned synthesize methyl acrylic acid glycidyl ester, in order to make the accurate of constant flow pump control flow, before using micro-reactor apparatus, also comprise the step that it is calibrated, described being calibrated to uses absolute ethyl alcohol to carry out.
In the method for above-mentioned synthesize methyl acrylic acid glycidyl ester, can be through the ratio calculating product reaction time of time-delay reaction channel volume with flow rate of liquid.Calculating formula is following:
T=V/ (u
Constant flow pump I+ u
Constant flow pump II)
Wherein t is the reaction time, and V is time-delay reaction channel volume, and u is the constant flow pump flow velocity.
Synthesize methyl acrylic acid glycidyl ester reaction equation is following:
Raw material used in the present invention is liquid or is the solid matter that can be dissolved in raw material that the product of generation also is a liquid, is suitable for micro-reactor apparatus of the present invention.
Micro-reactor apparatus of the present invention has the advantage of process intensification; In the esterification by ring opening course of reaction; Methacrylic acid solution and epoxychloropropane are fully mixed in the short time at the utmost point, and guaranteed the timely transmission of heat of reaction, prevented the generation of the limited and polymerization side reactions that rate of heat transfer slowly causes of long because of the reaction time, the mixed effect of traditional handicraft; Reduce impurity in products content, improved the conversion ratio of methacrylic acid.In the ring-closure reaction process; Owing to be the profit two phase reaction; Microreactor can mix the esterification by ring opening product that is oily with the rapid and uniform that sodium hydrate aqueous solution reaches on the minute yardstick; Improved mixed effect greatly, made to be reflected in very short time and accomplish, avoided product in the popular response system, inhomogeneously to prolong the reaction time, caused product hydrolysis and side reaction such as polymerization takes place under alkali condition because of stirring.Because the stirring of having avoided existing in the popular response is mixed and the restriction of system heat transfer aspect, and combined coefficient is improved greatly, and is fit to continuously synthetic.
Therefore, the present invention has the following advantages:
Micro-reactor apparatus of the present invention, material pumps into through constant flow pump, has guaranteed the accurate and easy and safe to operate of material metering; The state that conveying and the transfer of material in reaction system is in sealing makes the operation safety and environmental protection; Also can carry out online in real time to relevant technological parameter and regulate, technological parameter can show intuitively, is beneficial to the control to synthesis technique.
Micro-reactor apparatus of the present invention is applied in the synthesize methyl acrylic acid glycidyl ester, and the purity of the feed stock conversion of its two-step reaction and product GMA is high than traditional handicraft; The building-up process continued operation, saving reaction time and energy resource consumption, reaction process amplify easy; Need not conventional chemical reaction devices such as agitated reactor and condenser, equipment input and maintenance cost are low relatively; Raw material is directly pumped into by constant flow pump, has made things convenient for to add the link that feeds intake, and has strengthened the security of operation; Process conditions control is easy, can online process conditions be adjusted at any time on demand.
Description of drawings
Accompanying drawing 2 width of cloth of the present invention,
Fig. 1 is the micro-reactor apparatus structure chart of present embodiment 1;
Fig. 2 is the micro-reactor apparatus structure chart of present embodiment 2;
Wherein, 1, head tank, 2, the thermostatical oil bath, 3, receiver, 4, micro-mixer, 5, the time-delay reaction channel, 6, constant flow pump.
The specific embodiment
Following non-limiting example can make those of ordinary skill in the art more fully understand the present invention, but does not limit the present invention in any way.The employed micro-mixer model of this instance is that SIMM-V2 is German IMM manufactured.Raw material epoxychloropropane used in the present invention is pure for analyzing, and Tianjin recovery fine chemistry industry research institute produces; Methacrylic acid is a technical grade, and the Ningbo chemical industry Co., Ltd of rising produces; NaOH is pure for analyzing, and Tianjin recovery fine chemistry industry research institute produces; Methenamine is pure for analyzing, and Yixing City Chemical Reagent Plant No.2 produces; MEHQ is a chemical pure, and Chemical Reagent Co., Ltd., Sinopharm Group produces.
Adopt the GC assay products among the present invention, its test condition: gas chromatograph is upright 9800 types of good fortune; Work station reaches N2000 for Zhejiang intelligence; Chromatographic column: fused-silica capillary column 30m * 0.32mm * 0.5 μ m; Column type: FFID; Column temperature: 160 ℃; Detector temperature: 250 ℃; Temperature of vaporization chamber: 270 ℃; Detector: flame ionization ditector.
Embodiment 1
The present invention combines accompanying drawing 1 to describe.The head tank I101 of micro-reactor apparatus through constant flow pump I601 link to each other with micro-mixer 4, head tank II102 links to each other with micro-mixer 4 through constant flow pump II602, the opposite side of micro-mixer 4 reaction channel 5 that passes through to delay time links to each other with discharge tank 3; Micro-mixer 4 is fixed in the thermostatical oil bath 2 with time-delay reaction channel 5.The diameter of described time-delay reaction channel 5 is 3.175mm, and length is 2m, and its material is a stainless steel.The channel diameter of described micro-mixer 4 is 50 μ m.
The present invention combines accompanying drawing 2 to describe.The head tank I101 of micro-reactor apparatus through constant flow pump I601 link to each other with micro-mixer I401, head tank II102 passes through constant flow pump II602 and links to each other with micro-mixer I401; The opposite side of micro-mixer I401 links to each other with micro-mixer II402 through time-delay reaction channel I501, and micro-mixer I401 and time-delay reaction channel I501 are fixed among the thermostatical oil bath I201; Described head tank III103 links to each other with micro-mixer II402 through constant flow pump III603; The opposite side of micro-mixer II402 links to each other with receiver 301 through time-delay reaction channel II502, and micro-mixer II402 and time-delay reaction channel II502 are fixed among the thermostatical oil bath II202.The diameter of described time-delay reaction channel 5 is 3.175mm, and length is 2m, and its material is a stainless steel.The channel diameter of described micro-mixer 4 is 50 μ m.
Use the micro-reactor apparatus of embodiment 1 to come the synthesize methyl acrylic acid glycidyl ester.Concrete steps are following:
1. esterification by ring opening reaction:
Use absolute ethyl alcohol that micro-reactor apparatus is calibrated; Feed absolute ethyl alcohol pipeline is washed, the inspection pipeline has or not the seepage situation; With the 455g methacrylic acid solution, 7.63g methenamine and 3.30g MEHQ mix, and wait not have the solid insoluble matter, join among the head tank II102; The 634.8g epoxychloropropane is joined among the head tank I101; When the temperature of thermostatical oil bath 2 rises to 90 ℃; I601 opens with constant flow pump; The control flow velocity is that 2.2mL/min and constant flow pump II602 open, and the control flow velocity is 2.6mL/min, and liquid gets in the micro-mixer 4 and mixes; After the reaction, light yellow oily product I flows in the discharge tank 3 in time-delay reaction channel 5.
Product I is 70～80% through the conversion ratio that GC analyzes its methacrylic acid.
2. ring-closure reaction:
Use absolute ethyl alcohol that micro-reactor apparatus is calibrated; Feed absolute ethyl alcohol pipeline is washed, the inspection pipeline has or not the seepage situation; Product I is joined among the head tank I101; Mass percentage concentration 21%, 1.1L sodium hydrate aqueous solution are joined among the head tank II102; When the temperature of thermostatical oil bath 2 rises to 40 ℃, open constant flow pump I601 and constant flow pump II602, the control flow velocity is 6.0mL/min, enters into micro-mixer 4 and mixes, and after reacting in the inflow time-delay reaction channel 5, the product II that obtains gets in the discharge tank 3;
3. product II is changed in the separatory funnel and separate, get oil reservoir, be washed with distilled water to neutrality, anhydrous sodium sulfate drying obtains GMA.
It is＞95% that GMA is analyzed its purity through GC; Yield: (by methacrylic acid)＞80%.
Use the micro-reactor apparatus of embodiment 2 to come the synthesize methyl acrylic acid glycidyl ester.Concrete steps are following:
Use absolute ethyl alcohol that micro-reactor apparatus is calibrated; Feed absolute ethyl alcohol pipeline is washed, the inspection pipeline has or not the seepage situation; With the 455g methacrylic acid solution, 7.63g methenamine and 3.30g MEHQ mix, and wait not have the solid insoluble matter, join among the head tank II102; The epoxychloropropane of 634.8g is joined among the head tank I101; With 21%, the 1.1L sodium hydrate aqueous solution joins among the head tank III103; When the temperature of thermostatical oil bath I2 rises to 90 ℃, when the temperature of thermostatical oil bath II202 rises to 40 ℃, with constant flow pump I601; Constant flow pump II602 and constant flow pump III603 open, and the control flow velocity is respectively 2.2ml/min, 2.6ml/min; 4.8ml/min; Liquid gets into successively among the micro-mixer I401 and mixes, and in time-delay reaction channel I501, after the reaction, enters into micro-mixer II402 afterwards and mixes with sodium hydrate aqueous solution; After reacting among the inflow time-delay reaction channel II502, the product II that obtains gets among the discharge tank I301;
Product changed in the separatory funnel separate, get oil reservoir, be washed with distilled water to neutrality, anhydrous sodium sulfate drying obtains GMA.
It is＞95% that GMA is analyzed its purity through GC; Yield: (by methacrylic acid)＞80%.
Claims (9)
1. a micro-reactor apparatus is made up of a unit at least; Described unit comprises thermostatical oil bath (2) and discharge tank (3) and at least two head tank I (101), head tank II (102); Also comprise micro-mixer (4) and time-delay reaction channel (5); Described head tank I (101) through constant flow pump I (601) link to each other with micro-mixer (4), head tank II (102) passes through constant flow pump II (602) and links to each other with micro-mixer (4); The opposite side of micro-mixer (4) links to each other with receiver (3) through time-delay reaction channel (5), and time-delay reaction channel (5) is fixed in the thermostatical oil bath (2).
2. a kind of micro-reactor apparatus according to claim 1 is characterized in that described micro-mixer (4) is fixed in the thermostatical oil bath (2), and the channel diameter of its micro-mixer is 50 μ m～600 μ m.
3. a kind of micro-reactor apparatus according to claim 1 and 2, the diameter that it is characterized in that described time-delay reaction channel (5) is 1.59mm～6.35mm, length is 30cm～500cm.
4. a kind of micro-reactor apparatus according to claim 3, the material that it is characterized in that described time-delay reaction channel (5) is a stainless steel.
5. according to claim 1 or 4 described a kind of micro-reactor apparatus, it is characterized in that described receiver (3) is the micro-mixer in discharge tank or next the said unit.
6. a kind of micro-reactor apparatus according to claim 5; The head tank I (101) that it is characterized in that described micro-reactor apparatus through constant flow pump I (601) link to each other with micro-mixer I (401), head tank II (102) passes through constant flow pump II (602) and links to each other with micro-mixer I (401); The opposite side of micro-mixer I (401) links to each other with micro-mixer II (402) through time-delay reaction channel I (501), and micro-mixer I (401) and time-delay reaction channel I (501) are fixed among the thermostatical oil bath I (201); Described head tank III (103) links to each other with micro-mixer II (402) through constant flow pump III (603); The opposite side of micro-mixer II (402) links to each other with receiver (301) through time-delay reaction channel II (502), and micro-mixer II (402) and time-delay reaction channel II (502) are fixed among the thermostatical oil bath II (202).
7. the method for a continuous synthesize methyl acrylic acid glycidyl ester comprises esterification by ring opening reaction and ring-closure reaction, it is characterized in that said being reflected in the described micro-reactor apparatus of claim 1 carry out.
8. the method for a kind of continuous synthesize methyl acrylic acid glycidyl ester according to claim 7 is characterized in that described method step is following:
1. the esterification by ring opening reaction is synthetic:
A joins epoxychloropropane among the head tank I (101); With methenamine and MEHQ be dissolved in the methacrylic acid mixture I, its mixture I is joined among the head tank II (102); Wherein, Epoxychloropropane and methacrylic acid in molar ratio 1.3～1: 1 feeds intake; The addition of methenamine is 0.5～1.0% of methacrylic acid and an epoxychloropropane gross mass, and the addition of MEHQ is 0.1～0.5% of methacrylic acid and an epoxychloropropane gross mass;
When b rises to 70～100 ℃ with the temperature of thermostatical oil bath (2); Open constant flow pump I (601) and constant flow pump II (602); Flow velocity is 0.5ml/min～20ml/min; Enter into micro-mixer (4) and mix, inflows diameter is that 1.59mm～6.35mm, length are that the time-delay reaction channel (5) of 30cm～500cm reacts, in the product I entering discharge tank (3) that obtains;
2. ring-closure reaction:
A joins product I among the head tank I (101); With mass percentage concentration is that 10%～30% sodium hydrate aqueous solution joins among the head tank II (102); Wherein, NaOH and product I in molar ratio 1.0～1.1: 1 feeds intake;
When b rises to 40 ℃ with the temperature of thermostatical oil bath (2), open constant flow pump I (601) and constant flow pump II (602), enter into micro-mixer (4) and mix, flow into time-delay reaction channel (5) and react, the product II that obtains gets in the discharge tank (3);
3. product II is separated, get oil reservoir, washing is to neutral, and drying gets GMA.
9. the method for a kind of synthesize methyl acrylic acid glycidyl ester according to claim 8 also comprises the step that it is calibrated before it is characterized in that using micro-reactor apparatus, and described being calibrated to uses absolute ethyl alcohol or ethyl acetate to calibrate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102757409A (en) * | 2012-07-19 | 2012-10-31 | 湖南罗比特化学材料有限公司 | Preparation method of glycidyl acrylate |
| CN104086415A (en) * | 2014-07-18 | 2014-10-08 | 南京工业大学 | Method for preparing acetyl tributyl citrate by utilizing micro reaction device |
| CN104707547A (en) * | 2015-02-13 | 2015-06-17 | 清华大学 | Method for synthesizing polyvinyl butyral by using micro reaction system |
| CN108707126A (en) * | 2018-07-03 | 2018-10-26 | 山东柳湾新材料有限公司 | Using the method for microchannel reaction unit synthesizing methyl glycidyl acrylate |
| CN109762103A (en) * | 2019-01-22 | 2019-05-17 | 贵州微化科技有限公司 | A kind of micro- reaction method and device continuously preparing low dispersed acrylic resin |
| CN110075773A (en) * | 2019-05-31 | 2019-08-02 | 常州瑞曦生物科技有限公司 | The method of its synthesis benzocainum of micro-reactor apparatus and application |
| CN111617711A (en) * | 2020-06-15 | 2020-09-04 | 辽宁石化职业技术学院 | Microreactor and diarylethane preparation method based on microreactor |
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| CN115872952A (en) * | 2021-09-28 | 2023-03-31 | 佳化化学(上海)有限公司 | Preparation method and system of glycidyl methacrylate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102757409A (en) * | 2012-07-19 | 2012-10-31 | 湖南罗比特化学材料有限公司 | Preparation method of glycidyl acrylate |
| CN102757409B (en) * | 2012-07-19 | 2014-07-16 | 湖南罗比特化学材料有限公司 | Preparation method of glycidyl acrylate |
| CN104086415A (en) * | 2014-07-18 | 2014-10-08 | 南京工业大学 | Method for preparing acetyl tributyl citrate by utilizing micro reaction device |
| CN104707547A (en) * | 2015-02-13 | 2015-06-17 | 清华大学 | Method for synthesizing polyvinyl butyral by using micro reaction system |
| CN108707126A (en) * | 2018-07-03 | 2018-10-26 | 山东柳湾新材料有限公司 | Using the method for microchannel reaction unit synthesizing methyl glycidyl acrylate |
| CN109762103A (en) * | 2019-01-22 | 2019-05-17 | 贵州微化科技有限公司 | A kind of micro- reaction method and device continuously preparing low dispersed acrylic resin |
| CN110075773A (en) * | 2019-05-31 | 2019-08-02 | 常州瑞曦生物科技有限公司 | The method of its synthesis benzocainum of micro-reactor apparatus and application |
| CN111617711A (en) * | 2020-06-15 | 2020-09-04 | 辽宁石化职业技术学院 | Microreactor and diarylethane preparation method based on microreactor |
| CN113041966A (en) * | 2021-02-18 | 2021-06-29 | 浙江建业化工股份有限公司 | Method for preparing isopropylamine by using microfluidic technology and device used in method |
| CN113041966B (en) * | 2021-02-18 | 2022-10-28 | 浙江建业化工股份有限公司 | Method for preparing isopropylamine by using microfluidic technology and device used in method |
| CN115872952A (en) * | 2021-09-28 | 2023-03-31 | 佳化化学(上海)有限公司 | Preparation method and system of glycidyl methacrylate |
| CN113845495A (en) * | 2021-10-20 | 2021-12-28 | 清华大学 | Continuous synthesis method of two-stage glycidyl neodecanoate |
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Application publication date: 20120718 |